Preparation of nitrogen compounds.



E. H. MEYER @L J. M. A. STILLBSEN.

PREPARATION 0F NITROGEN COMPOUNDS. APPLICATION FILED sng'r. 15l 190s. RBNBWED AUG. 2, 1910.

982,288, Patented Jan. 24, 1911.

@subjects off the UNITED smrnsrfafrnn'r'-oFFioE.:

EINAR Hononmrns MEYER AND JOB MOETEN AUGUST STILLESEN, or NIAQARAF'ALLS/ cEN'rnE, ONTARIO, CANADA.

Pnnrana'rron or nrrROGENcc-)MPOUNDS Svpecication of-Letters' Patent. 'Patented-Jan 24,1911

Appie-ation ieaseptember'is, 150s, serii ne. 453,113.' neiewea Auguste; 191e.` serial 11a-575,180.

To whom 'it-moy coiwer'n: i d that we', EINAR HoNonA'rUs MEYER and Ontario and Dominion of Canada, have in l '-in `Preparation of Nitrogen Com-v clear, and exact specication.

This invent-ion'rel tes to electro-chcinis =try, 'and has'aiticular reference to the manufacture o nitrogen compounds, such f of the coal consistingof nitrogen, carbon difor instance, as lime nitrogen, etc.

More particularly, the invention relates to a process for the preparation oflime' nitrogen without free carbon. A

In preparing calcium carbid in th'eelectric furnace,calciumv oxid is' treated with an exthe evolution of ca rbon monoxid. In order to prepare linie nitrogemfwe take' calcium cess of carbon, to`fojrm calciiimcarbid'with Vcarbid'and treat'it in the presence of a flux and, heatgivitli' nitrogen, toget ver with carbon dioxid, to forni'a resultan product containing approximately thirty-five per cent.

presence of a flux which limestone mixed with coal in the desired proportion, according as calciuin.- car.

j to lime and carbon by heat from gas burners lmixediwith the desired yproportion of of nitrogen.

It is an object othis invention toprepare lime 'nitrogen and ,other compounds containinga larger percentage of combined nitrogen than hasheretoforebeen obtained by treating calcium carbid preferably inthe tions of nitrogen and carbon dixid, Whereby the free carbon heretofore present in lime nitrogen-willbe ox'idizedby the carbon di-4 oxid to carbon monoxi'd, which, beiiiga gas, will i The invention will be more drawing.

'1 represents an electric furnace,`\vherein calcium carbid is produced b v the action of theA electric arc. In order to obtain .lime

bon, a limestone retort 2 is provided in bid or calcium is to be prepared, and burned JOB MORTEN AUcs'r S'i1ii1.nsi`;n,4 King 'of Norway, residing at' through a drier 5,' to remove I ing lime water,

and the liin'e Water 'tank 6 "removes the carbon=d1ox1d, so -theA remaining gas will con-V Athat-is tO sa lime nitrogen Without ee carbon, itis desirable yto prol.carbon dioxid the proportion of. carbon with determined proporpass ofi", .leaving -tlie' resulting lime 'ni'A A.trogen without free carbon. nace, which' may -b'e heated' fully under-'- stood'fin connection f with the description of the apparatus employed, as shown in the ac,- companying The 'gas'usedis a mixture of" carbon inonoxid -from the carbid furnace Awith air,

air and acetylene or other suitable gas, so

combustion of the gas is ob# tained in the retort 2, hydro-carbone which may be lcontained in'. the coal itsell From the retort,2 the lime and carbon are .discharged into the` electric furnace 1, 'either for producing calciunicarbid `or .for producing pure calcium, accordj1n g to the proportion 'ofcarbon used. The

gaseous products lof-the combustionv yoi? the gas at .the burners 'and volatile constituents oxid and Water, arecondu'cted by a` pipe i the Water' of combustion and thence to altank 6 containor some, ot-lierineans for separating carbon dioxid .so-asl to leave pure nitrogen. The drier 5 .removes the water,

sist of pure nitrogen, .Which-'passes from the` tank 6, .through apipe 7 containingra 'reguv lating-valve 8. n,

For the preparation of .pure lime nitrogen,

the ad- A mixture of vide a source of carbon dioXid separate from the carbon dioxid given oiifromfthe retort E?, since by the use'ofaseparate sourcefof di. 'oxid admitted tothe. furnace 12 can be regulated'in accordance witlithe particular linie nitrogen; to be produced, 'it being possible, as before stated, to regulate the proportion 'of nitrogen by niea'nsof the'valve 8. l

16 represents -fan ordinarylimestone f nr-j by burners 1T for forming carbonv dioxid, which will ,pass through a regulatingvalve 18, and thence by pipeA 10 to the Afurnace 12. The .-calciuinA carbid is charged'into the furnace through a suitablecharging door as l15, and the furnace is heated byburners 13. v Also, a flux of calcium fluorid or-ci'yolite, or both, is

provided, and means' fOr-.thoroughlymixing the gases '.with the' meltedy carbid andf flux.'

The typical reaction may.' stated. asffolf loW's caoifarecogscacmaco. j. r-I`he flux' does'not react Athe. carbid,

"but has'. 'the-' funct o'n" ofI promoting 'and 'together with .the'

at all, only on the outside of the .particles,'-

l -romafseparate source'such as the retort 16."

'With the nitrogen* Without the flux, even ,K1 yield of lime nitrogen, by yreason yof the ment'vvithl carbon dioxid, the lime nitrogen through' it, but the carbon dioxid is reduced 'bon,rand having a percentage of less than ofthis,inventionkthe product -Will contain :about thirtyeve per cent., of combinedA nitrogen. This is a considerable improve-ment in .the manufacture ,of nitrogen compounds, -sincethereby is produced a pure compoundv-freefof, ca`rbon,Whether of lcalcium or some practice, and the product it is desired `to- .j -nitrogen ,free of. carbon, 1400 degrees C. has

'ofl calcium nitrid, 1000 degrees C. has been 1furnace lsoasto'maintain the reactions under the proper conditions.v Vlnle we have;

.described b-yi preference a"sepa`ralte source nitrogen r-Without passingy 1through the;l tank, 46', though the. proportion of -carbon- .dio 'id 2 eea,

assisting 'the reaction. Without 'the flux," the nitrogen combines with the carbid,`-it

leaving the insidey unchanged. 'I`he'carbidr 1s, so to-say, indiii'erent'tothe combination though the temperature be raised as high asf- 1200 to 1500 degrees. Besides the greater flux, it is' non-hygroscopic. Without 'treatcontains free carbon particles disseminated by the free carbonunder the influence of heat, to carbon monoxid, Which passes on? as a gas, leaving the lime nitrogen vtree oty carbon. The result of this process is that Whereas We .haye heretofore proposed to produce lime nitrogen contaningfree car-v thirty vper cent. of nitrogen, bythe process other metal.

`resulting'` product. iv; .y .p 3. The process ofpreparing llme nitrogen consistingiin treating 'calcium carbid with nitrogen, and eliminating carbonffrom the resulting productyby oxidation'.

4. The process ofpreparing lime4 nitrogen consisting in treating calcium carbid with nitrogen, fandeliminating carbon from theI resulting productAly by oxidation with carbon diolxidl.,v 't

5,` The process o preparing linie nitrogen consisting in Y.treating vcalcium rar-bid with nitrqgemrand, yeliminating carbon from the resulting product by oxidation with a detei-minedv proportion of carbon dioxid.

v(3; 'The-process' of preparing linie nitrogen consisting in treating'calcium carbid with nitrogenl the presen'cofal iiu'x, and eliininating' carbon from' .the resulting product.

r The temperature ofthe furnaceniifillbf.:iti-7. The processf'ofpreparinglilnentlogen lcourse be yregulated'or Variadas *maybel desired according Ito the conditions of actual obtain., For the production of pure lime beenfound suitable, and for the production foundfsatisfactory. It will bennderstoodl that the gases shouldgbe introduced intothe furnace under-,av slight pressure, and the escape of 4thexevolved gases will be controlled through", av suitable `Vent` yfrom the Yconsistin'gfin'itrea'tiiig calcium carbid `with nitrogen in the presencel of" al' tiuxf and eliminating carbon1 from the f resulting product, by treatment with carbon dioxid.

8. The process ,of preparing lime lnitrogen consisting in lreducinglimestone t'o lime by combustion, of a gaswith `air`,"h`eating the lime-'in the presen'ceoi:l carbon `to formi carbid, and treating theb'arbid niithth nitro.- igen from 'the coinbnstiongases 'and 'carbon dioxid to 'produce a compound o'linie rarbon andnitrog'el'i'freev of uncombined carbon.

`9. The process fremoving fi-'eet carbon from compoundY comprising' coinlbined cal cium,"carbon and nitrogenconsisting ,in heatof' carbon dioxidfor the production ottv pure fing such compound 'ii'ith carbfongdipxidnlstood ,that the carbon ldioxid troni/tire:firew tortl furnace I2 fmay be .used mixed' "with cannot inthis mannerbe as 'closely propo; tioned-to the chemical' requlrements and' equivalents `as by producing carbon dioxid lsid; apparatus in various ]:iarti'culars'A` Without departing thereroirno nitrogenoin the 'presence of af 1ng; a. f luorld, and' eliminatni l0. The process of preparing liniel nitrogen" conisting in treating calciuml'rarbidwith'l Y uenipiirree canlipn therefromby'onidation, u

ll-'The herein described process/consist- `i151 lngI in treati'ngcalciun'i carbid n'if'tlrnitrogein j and carbon dioxid inthe'presence of comprising afluorid.l 'j ,1 l il `12.]'j'hei,herein described proce consisb "i ing in -treatingi'gheated calcium. carbidl and`f1'2'0 alux withj nitrogen and carbon -Atlioxid .,jxntestimony 'whereofiire aiiix our signa.- Qtures, inipresence of twowitnesses.

rirlnuorolurus i1Ei'Ei:..-p.

."Witnesses':1 t f VVLLEIGHBAU, `J. E. Riel-manson. 

